温和条件下催化合成纳米镧系金属氢化物及纳米NaH高活性研究
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摘要
1．本论文首次提出一种在温和条件下催化合成纳米尺寸的镧系金属氢化物的方法，介绍在常温常压下，镧、钕、钐、镝、镱五种镧系金属在四氢呋喃(THF)溶剂中，催化剂作用下与氢气直接化合形成相应的纳米尺寸的镧系金属氢化物。借助透射电镜(TEM)、X射线粉末衍射(XRD)和BET法对其产物进行了表征。TEM测试表明所得产物的平均颗粒直径在20-40nm范围内。同时对合成中多种反应参数的影响进行了考察。
1 Lanthanide hydrides (M = La, Nd, Sm, Dy and Yb) can be prepared easily by the direct hydrogenation of lanthanide metals catalyzed by TiCl4 in tetrahydrofunan (THF) under normal pressure. The rate of hydrogenation decreased with increasing atomic number of lanthanides. Transmission electron micrographs showed that the resulted lanthanide hydrides were in the form of nanoparticles with an average primary particle size around 20-40 nm. The structures of their hydrides were characterized by the X-ray powder diffraction (XRD) method. And the effects of the various parameters to the catalytic synthesis reaction of lanthanide hydrides were discussed.
1 Lanthanide hydrides (M = La, Nd, Sm, Dy and Yb) can be prepared easily by the direct hydrogenation of lanthanide metals catalyzed by TiCl4 in tetrahydrofunan (THF) under normal pressure. The rate of hydrogenation decreased with increasing atomic number of lanthanides. Transmission electron micrographs showed that the resulted lanthanide hydrides were in the form of nanoparticles with an average primary particle size around 20-40 nm. The structures of their hydrides were characterized by the X-ray powder diffraction (XRD) method. And the effects of the various parameters to the catalytic synthesis reaction of lanthanide hydrides were discussed.
引文
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32. Zhang Y K, Liao S J, Fan Y H, et.al., J Nanoparticle Res, 2001, 3: 236.
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34．张源魁，中国科学院大连化学物理研究所博士学位论文，1997．
35. Fan Y. H., Liao S. J, Xu J. et al.. J. Catal., 2002, 205:284-289
36．范荫恒，廖世健，徐筠等，高等学校化学学报，1997,18：1683．
37．范荫恒，廖世健，徐筠等，催化学报，1998，P．389．
38. Kinkelin, E.; Fink, G.; Bogdanovic, B., Chem., Rapid Commun., 1986, 7.
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40．孙奉玉，吴鸣，李文钊等，催化学报(Journal of Catalysis)，1998，19(3)．
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42．张一平，乔志敏，廖世健，徐筠，余道容，中国申请专利95 110017，3．
43．王宏运，郭景坤，高濂，硅酸盐通报，1999，18．
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b. 冯新德，蒋德彰，雷永铭，高分子通讯，1965，7，112．
c. H.L.Needles, J.Polym.Sci., 1969, Part A-1, 7,1437.
62．张文明，中国科学院大连化学物理研究所硕士学位论文，1995．
63. W.Zhang, L.Zhang, S.Liao, Y.Xu and D.Yu, Chin.Chem.Lett., 1995, 6,839.
64．张文明，廖世健，徐筠，张一平，余道容，化学试剂，1995，17,71．
65．张莉，中国科学院大连化学物理研究所硕士学位论文，1994．
66. T.P.Burns and R.D.Rieke, J.Org.Chem., 1987, 52,3674.
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68. Idem, J. Mol. Catal., 1990,L1.
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71. Zhang, T-P.; Liao S-J.; XU, Y., Tetrahedron Lett., 1994,35.
72．张一平，徐筠，廖世健，中国专利申请，93，111152,8．
73. Y.Zhang, S.Liao ,Y.Xu and D.Yu, Chin. Chem. Lett., 1995,6,735.
74．郦海青，中国科学院大连化学物理研究所硕士学位论文，1996．
75. G.Hugel, Chimie and Industie Special No., 1929,128.
76. G.Hugel, Can. Chem. Met., 1929,13.
77. G.Hugel and J.Friess, Bull.Soc.Chim.France, 1931, 49:1042.
78. G.Hugel and J.Friess, Ann. Combustibles Liquides, 1931,6:1109.
79. F.W.Bergstrom and J.F.Carson, J,Am.Chem.Soc., 1941,63:2935.
80. L.H.Slaugh, J.Org.Chem.,1967,32:108.
81. Shell Internationale Research Maatschappij, N.V.Neth.Appl., 1965, 171.
82. C. Qian, Z. Xie and Y.Huang, J. Organomet. Chem., 1987,285.
83．张一平，中国科学院大连化学物理研究所博士学位论文，1990．
84. Y.Zhang, S.Liao and Y.Xu, J. Organomet. Chem., 1990, 69, 382.
85. Seiman, J.R., US Pat. 1990,4,910,353.
86．范荫恒，廖世健，李伟娜等，应用化学，2001，18(5)．
87．范荫恒，廖世健，李伟娜等，Chinese Journal of Chemistry(待发表)．
88．孙琪，廖世健，徐筠等，高等学校化学学报，1996，17：1441．
89. Qi Sun, Yinheng Fan, Shijian Liao et al. Polymer, 2001,42.
90. Daniel L. F., Colby A. F. Jr.. Metal Nanoparticles Synthesis Characterization and Applications[M], MARCEL DEKKER INC New York and BASEL, 2002
91. Katharina Landfester Adv. Mater.[J], 2001, 13:765
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